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October

IS

3812

(Part

W’T%%7m

Indian

Standard

PULVERIZED

FUEL ASH — SPECIFICATION

PART 1

FOR USE AS POZZOLANA

IN CEMENT,

CEMENT

MORTAR

AND CONCRETE

(Second

Revision )

ICS 91.100.10

1) :2003

2003

BUREAU

MANAK

OF

BHAVAN,

0

BIS 2003

INDIAN

9

NEW

BAHADUR

DELHI

STANDARDS

SHAH

110002

ZAFAR

MARC

Price Group

5

Cement

and Concrete

Sectional

Committee,

CED

2

FOREWORD

This Indian Standard

(Part

1) (Second

Revision)

was adopted

by the J3ureau of Indian

Standards,

after the draft

finalized by the Cement.and Council.

Concrete

Sectional

Committee

had been approved

by the Civil Engineering

Division

Pulverized fuel ash is a residue resulting from the combustion of ground or powdered

or sub-bituminous coal (lignite). About 80 percent of the total ash is finely divided

as fly

ash. It is sometimes referred as chimney ash and hopper ash. The balance about 20 percent of ash gets collected

is

collected and stored in dry condition. When fly ash alone or alongwith bottom ash is carried to storage or deposition lagoon or pond in the form.of water sluFFy and deposited, it is termed as pond ash. Whereas if fly ash,

alone or alongwith bottom ash is carried mound ash.

as

with

or crushed bituminous coal

and get out of boiler along

is termed

ash.

Fly ash

it is termed

flue gases

and is collected

by suitable

technologies.

out by suitable

to a storage

This ash generally

technologies

and is

and in this standard

referred

as bottom

and deposited,

at the bottom of the boiler and is taken

or deposition

site in dry form

PLlIverized fuel ash is available in large

power stations and industrial plants using pulverized or crushed or ground coal or lignite as fuel for boilers. The effective use of pulverized fuel ash as a pozzolana in the manufacture of and for part replacement of cement, as an admixture in cement, cement mortar and concrete, lime pozzolana mixture and products such as fly ash lime bricks, autoclave aerated concrete blocks, etc, have been further established in the country in recent years. Recent investigations of Indian pulverized fuel ashes have indicated greater scope for their uti Iization as a

construction material. Greater utilization of pulverized fuel ash will lead to not only saving of scarce construction materials but also assist in solving the problem of disposal of this waste product. The recent investigations have

also indicated the necessity to provide proper collection methods

uniformity which are prime requirements of fly ash for use as a construction material.

quantities

in the country

as a waste

product

from a number of thermal

for fly ash

so

as to yield

fly ash of quality

and

This standard was first published in 1966 in three parts to cater to the requirements of fly ash for three specific

uses: Part 1 covering use of fly ash as a pozzolana, Part 2 covering use of fly ash as an admixture for concrete, and Part 3 covering use of fly ash as fine aggregate for mortar and concrete. The Sectional Committee responsible for the formulation of this-standard subsequently felt that the performance of fly ash as a pozzolana or an admixture or a fine aggregate, was complementary and not separable and hence requirements of fly ash for these uses

standard was, therefore, revised in 1981 by combining the three

should be covered by a single standard. This

parts into a single standard, also incorporating the modifications found necessary based on the experience gained with the use of earlier standard. This revision classified fly ash in two grade, Grade 1 for incorporation in

cement, mortar and concrete and in lime pozzolana mixture, and for manufacture of Portland pozzolana cement, and Grade 2 for incorporation in cement, mortar and concrete and in lime pozzolana mixture.

Improvements have taken place over time in combustion technologies and ash collection technologies. These technological developments have resulted in improvement in ash qualities; specially the fineness and loss of ignition. Technologies have also been developed for a large number of utilizations of wide range of pulverized fuel ash. Application of technologies in the collection, transportation and deposition of ash have also resulted in availability of pulverized fuel ash in four forms, namely, fly ash, bottom ash, pond ash and mound ash. Though the last revision of the standard pertained only to fly ash, number of important applications of fly ash were left uncovered. The Sectional Committee, therefore, felt necessary that a comprehensive specification should be brought out. Separate Indian Standards for fly ash for use in different end applications such as l~me pozzolana mixture applications, sintered applications, geotechnical applications and agricultural applications are alsobeing developed.

This

revision

intends

to bring

out the standard

for pulverized

fuel ash in two parts.

The other

part is:

Part 2

For use as admixture

in cement

mortar

and concrete

(Continued

on third cover)

IS 3812

(Part

1) :2003

Indian

Standard

PULVERIZED

FUEL ASH — SPECIFICATION

PART 1 FOR USE AS POZZOLANA

IN CEMENT,

CEMENT

MORTAR

AND CONCRETE

(Second

1 SCOPE

1.1 This

the physical and chemical requirements of pulverized fuel ash for use as pozzolana for manufacture of cement

and for part replacement of cement in cement mortar and concrete.

standard

(Part

1) covers

the

extraction

and

1.2 Pulverized

fuel

ash

to

be

used

as pozzolana

in

cement, cement mortar and concrete in accordance with this standard shall be fly ash only which may be either in as collected condition or beneficiated, segregated or processed.

2

REFERENCES

The

which

provisions

standmds

through

given

in Annex

in

provisions

constitute

At the time of publication,

A contain

this

reference

of this standard.

text,

Revision

aluminate

)

hydrates.

NOTE — To evaluate this fraction, the total calcium oxide contents is to be reduced by the fraction calculated as calcium carbonate (CaC03), based on the measured carbon dioxide (COJ content and the fraction calculated as calcium sulphate (CaS04), based on the measured sulphate (S03) content, disregarding the S03 taken-up by alkalis.

3.5

Fly Ash — Pulverized

fielash

extracted

from flue

gases by any suitable process

such

as

by

cyclone

separator or electro-static

precipitator.

3.6 Bottom

the bottom

Ash Pulverized

fuel ash collected

of boilers

by any suitable

process.

from

3.7 Pond

in any proportion and conveyed in the slurry and deposited in pond or lagoon.

Ash Fly ash or bottom

ash or both mixed

of water

form

3.8 Mound

Ash Fly ash or bottom

ash or both mixed

the editions indicated

were

valid.

All

standards

are

in any proportion

and conveyed

or carried

in dry form

subject

to revision,

and

parties

to agreements

based

and deposited dry.

on this standard

are

encouraged

to

investigate

the

possibility

of applying the most recent editions of the

4 EXTRACTION

OF

FLY

ASH

 

standards

indicated

in Annex

A.

4.1 Fly ash may be extracted

from flue gases of ground

3 TERMINOLOGY

For the purpose of this standard, the definitions given below shall apply and for other terms definitions given in 1S 4305 shall apply.

3.1 Pulverized

of ground or pulverized

boilers. It can be fly ash, bottom ash, pond ash or mound ash.

Fuel Ash Ash generated

or crushed

by burning

fired

coal or lignite

3.2 Siliceous Pulverized Fuel Ash Pulverized fuel

ash with

reactive

calcium

oxide

less than

10 percent,

by mass.

Such

fly

ash

are

normally

produced

from

burning

anthracite

or

bituminous

coal

and

has

pozzolanicproperties.

3.3 Calcareous

fuel ash with reactive calcium oxide not less than

Pulverized

Fuel

Ash Pulverized

10 per~ent

by

mass.

Such

fly

ash

are

normally

or pulverized by any suitable

or crushed coal or lignite fired boilers

such as, by cyclone separation

process;

or electrostatic precipitation;

bottom

ash

from

the

boilers

shall

not

be

added

to

the

fly

ash.

Fly

ash

collected

at later stages

of electrostatic

precipitator

are

finer than the fly ash collected

at

initial

stages

of

electrostatic

precipitator.

NOTE — For extraction details for other types of pulverized

fuel ash such as bottom IS 3812 (Part 2).

ash, pond

ash and mound

ash refer to

5

PROCESSING

BENEFICIATION,

OF

SEGREGATION

PULVERIZED

FUEL

AND

ASH

5.1 Fly

ash as collected,

if does

not

conforms

to the

requirements

of this standard

or if required

otherwise,

may

be

processed

andtor

beneficiated

andlor

segregated

to

modify

its

physical

or

chemical

characteristics.

 

produced from lignite or sub-bituminous coal and have

5.2 Appropriate technologies may be applied for

beneficiation, segregation and processing of fly ash to

both pozzolanic

and hydraulic

properties.

 

3.4

Reactive

Calcium

Oxide

(CaO) — That fraction

improve its properties,

such as lime reactivity,

loss of

of the calcium

oxide

which

under

normal

hardening

ignition, particle size distribution and any of other

condition can form calcium silicate hydrates or calcium

physical and/or chemical properties. Some of the

1

1S 3812

(Part

1) :2003

technologies that may be used are burning/removal of unburned carbon, sieving/grading of fineness, grinding/attrition for reducing particle size, thermal treatment and blending of fly ash of different qualities.

6 CHEMICAL

REQUIREMENTS

6.1 Pulverized

requirements

fuel ash, shall conform

given

in Table

1.

to the chemical

6.2 The

condition as mutual] y agreed. However,

condition, the moisture content shall not exceed

2 percent. All tests for the properties specified in 6.1 shall, however, be carried out on oven dry samples.

in case of dry

fly

ash

may

be

supplied

in

dry

or

moist

7 PHYSICAL

REQUIREMENTS

7.1 Pulverized fuel ash, when tested in accordance with the methods of test specified in IS 1727, shall conform 10 the physical requirements given in Table 2.

7.2 Uniformity

Requirements

In tests on individual samples, the specific surface, particles retained on 45 micron IS Sieve (wet sieving) and lime reactivity -value shall not vary more than 15 percent from the average established from the tests

on the 10 preceding samples or of all preceding samples

if less than

10.

7.3

specified in Table 2, mixes in which pulverized fuel ash is incorporated shall show a progressive increase in strength.

Notwithstanding

the

strength

requirements

test shall be-taken

as described

in 9 and shall be tested

in

accordance

with

6 and

7.

8.2

All tests

for the properties

of the pulverized

fuel

ash shall be carried

out

as it is supplied.

in case

the

pulverized fuel ash supplied is to be beneficiated

or

segregated or processed, the tests shall be carried out

only after benificiation, applicable.

as

segregation

or~rocessing

8.3 Independent

Testing

8.3.1 If the purchaser or his representati~e requires independent test, the samples shall be taken before or

immediately after delivery at-the option of the purchaser

or his representative, and the tests shall be carried outi

this

arranged by the purchaser in accordance with

standard. The supplier shall make available, free of charge, the pulverized fhel ash required for testing.

‘8.3.2 After a representative sample has been drawn,

tests on the sample shall be carried out as expeditiously

as possible.

9 SAMPLING

9.1 Samples

for Testing

and by Whom

to be Taken

A sample

purchaser or his representative, or by any person

appointed to superintend

the pulverized fuel ash is required or by the latter’s representative.

the work for purpose of which

or samples

for testing

maybe

taken

by the

8 TESTS

8.1 The sample

s]

No.

 

9.2 In addition

to the requirements

of 9.1, the methods

and procedure

of sampling

shall be in accordance

with

or samples

of pulverized

fuel ash for

IS

6491.

Table

1 Chemical

Requirements

 
 

(Ckwe

6.1)

 

Characteristic

Requirements

Method of Testj

Ref to

(1)

i)

ii)

iii)

iv)

v)

vi)

\ii)

viii)

~~

 

Siliceous

Calcareous

Annex

IS No.

Pulverized

Pulverized

Fuel

Ash

Fuel Ash

(2)

(3)

(4)

(5)

(6)

Silicon dioxide (Si02) plus ahsminium oxide (A1203) plus km oxide (FelOj) in percent by mass, A4in

70

50

IS 1727

Silicon dioxide (SiOz) in percent by mass, A4in

35

25

IS 1727

‘1Reactive silica in percent by mass, &fin

20

20

B

Magnesium oxide (MgO) in percent by mass, Max

5.0

5.0

IS 1727

Total sulphur as sulphur trioxide (S03) in percent by mass, &fox

3.0

3.0

1S 1727

Available alkalis as sodium oxide (NazO) in percent by mass, Mux

1.5

1.5

Is 4032

Total chlorides in percent by mass, Max

0.05

0.05

IS 124232

Loss on ignition in percent by mass, Mu

5.0

5.0

1S 1727

“Optional test. ~’For the purpose

of this test, wherever

reference

to cement

has been made,

2

it may be read as pulverized

fuel ash.

Table

2 Physical

 

IS 3812

(Part

1) :2003

Requirements

packed

in bags

at the plant

in a sample

shall

be equal

SI

No.

(1)

(Clause

Characteristic

(2)

7.1)

i)

Fineness-specific surface in m2/kg by Blaine’s perme- ability method, &fin

ii)

‘‘Particles

 

retained

on

45

micron

IS

sieve

(wet

iii)

iv)

sieving)

Lime reactivity

compressive

Nlmm3, Min

Compressive

28 days in N/mm*, Miss

in percent,

Max

Average

in

at

strength

strength

v) Soundness by autoclave test – Expansion G_ specimen in percent, Max

Requirements

(3)

320

34

4.5

Not

of

corresponding

cement

less than 80 percent

the

strength

of

plain

mortar cubes

0.8

NOTE — Fly ash of fineness 250 m2/kg (Mitr) is also permitted to be used in the manufacture of Portland pozzolana cement by intergrinding it with Portland cement clinker if the fly ash when grou’nd to fineness of 320 mzlkg or to the fineness of ttre resultant Portland pozzoiana cement whichever is lower, meets all the requirements specified in 6 and 7 of this standard.

‘‘ Omional

test.

to

applicable.

given

or

more

below:

than

15 kg,

The number

Batch Size

30

kg,

300

kg,

of bags in a sample

Sample

Size

600

as

shall be as

kg

100

to 150

20

151

to280

32

28.1 to 500

50

501 to

1200

80

1201

to 3200

125

3201

and over

200

The bags

in a sample

shall

be

selected

at random

(see IS 4905).

 

11.2.2 The number

of bags

in a sample

showing

a

minus

error greater

than 2 percent

of the specif~d

net

mass

shall

be not more

than

5 percent

of the bags

in

the sample.

in the sample

net mass

Also the minus

exceed

shall

of pulverized

fuel

error

4 percent

in none

of such bags

of the specified

ash in the bag.

NOTE — The matter given in 11.2.1 and 11.2.2 are extracts based on the Standards of Weights and Measures (Packaged Commodities) Rules, 1977 to which reference shall be made for full details. Any modification made in these Rules and’other related Acts and Rules would apply automat ical Iy.

9.3 Facilities

for

Sampling

and

Identifying

The supplier

shall

afford

every

facility,

and

shall

provide all Iabour and materials

the samples for testing the pulverized fuel ash and for

for taking

and packing

subsequent identification sampled.

of

pulverized

fuel

ash

10 STORAGE

Pulverized

fuel ash may be stored

in accordance

with

the recommendation

given

in IS 4082

for cement.

11.2.3 In case of-a wagon or truck load of 5 to 25 tonne, the overall tolerance on net mass of pulverized fuel ash shall be O to + 0.5 percent.

11.4 The

Standard

consignment

Mark.

may

also

be marked

with

the

12 MANUFACTURER’S

CERTIFICATE

The

pulverized fuel ash conform to the requirements of this standard, and if requested, shall supply a certificate to this effect to the purchaser or his representative.

manufacturer

shall

satisfy

himself

that

the

11 DELIVERY

in

bulk in suitable quantities mutually agreed upon between the purchaser and the supplier. Where so required by the purchaser, the pulverized fuel ash may also be supplied in bags (jute, jute-laminated, multiple paper or polyethylene lined) bearing the net mass (may be 15 kg, 30 kg, 300 kg, 600 kg as agreed to between that purchaser and the supplier), supplier’s name or registered trade-mark, if any. The tolerance on the mass of pulverized fuel ash in each bag or consignment shall be as mutually agreed upon between the purchaser and the supplier.

11.1 Supplies of pulverized fuel ash may

be made

.11.2 Tolerance Requirements

for

the

Mass

of

Pulverized Fuel Ash Packed in Bags

 

11.2.1

The

average

net

mass

of pulverized

fuel

ash

3

13

MARKING

13.1 Each bag/consignment

be clearly

information:

and-permanently

of pulverized

marked

fuel ash shall

with the following

a)

b)

c)

d)

e)

8

!3)

Identification

pulverized

Type of pulverized or calcareous.as

of

the

-manufacturer

of

fuel ash;

fuel ash, that is, siliceous applicable;

Form of pulverized

fuel ash,

that

is, fly

ash

and its minimum fineness as per Table 2;

Batch/Control

unit numbe~

Net mass;

Month

and year

of packing;

and

Any other

identification

mark

as required

by

the purchaser.

1S 3812

(.Part

1) :2003

13.2 BIS Certification

Marking

14 REJECTION

The pulverized

fuel ash may also be marked

with the

14.1 Pulverized

fuel ash may be rejected

if it does not

Standard

Mark.

comply

with any of the requirements

of this standard.

13.2.1 The use of the Standard Mark is governed by

14.2 Pulverized

fuel ash in bulk storage

for more than

the provisions of the Bureau of Indian Standards Act,

6 months

or

in bags

 

for

more

than

3 months

after

1986 and the Rules and Regulations made thereunder.

completion

of tests,

may

be retested

before use and

The details of conditions under which a licence for the

may be rejected,

if

it

fails

to

conform

to

any

use of the Standard Mark may be granted to manufacturers or producers maybe obtained from the Bureau of Indian Standards.

requirements

of this standard.

 
 

ANNEX

A

(Clause

2)

 

LIST

OF REFERRED

INDIAN

STANDARDS

IS No.

Title

IS No.

 

Tide

264:1976

Nitric acid (second revision)

 

265:1993

Hydrochloric acid ~ourth revision)

 

revision)

 

1070:1992

Reagent grade water (third revision)

4032:1985

Method of chemical analysis of

1727:1967

Methods of test for pozzolanic

 

hydraulic cement @rst revision)

 

2263:1979

materials @rst revision) Methods of preparation of indicator solutions ~rst revision)

4082:1996

4305:1967

4905:1968

6491:1972

12423:1988

Recommendations -on stacking and storage of construction materials and

components at site (second revision)

2316:1990

Methods of preparation of standard

Glossary of terms relating to

solutions for calorimetric and volumetric analysis (second revision)

pozzolana Methods for random sampling

3812

Pulverized fuel ash — Specification:

Methods for sampling fly ash

(Part

2):

2003

Part 2 For use as admixture in cement mortar and concrete (second

Methods forcolorimetric analysis of hydraulic cement

ANNEX

B

[Table 1, S1No. (iii)]

METHOD

OF TEST

FOR

REACTIVE

SILICA

B-1 REAGENTS

AND

SPECIAL

SOLUTIONS

B-1.1 Unless specified otherwise, pure chemicals of analytical reagent grade shall be employed in tests, and distilled water (see IS 1070) shall be used where the use of water as a reagent is intended. The following reagents -and special solutions of analytical reagent grades are required (see IS 2263 andIS2316).

B-1,1.1

Reagents

B-1.l.l.l

(conforming

Hydrochloric to IS 265).

acid

sp

gr

1.16

B-1.1.1.2 Sulphuric acid — sp gr 1.42 (conforming to IS 264).

B-1.1.1.3

4

Hj&ojluoric

acid — 40 percent.

B-1.l.

1.4 Sodium peroxide

solid.

B-1.1.1.5

Sodium

hydroxide

B-1.1.1.6

Sodium

carbonate

solid.

B-1.l

1.7

Sodium

chloride

solid.

B-1.l.2 Diiute Solutions of Reagents Prepare the following dilute solutions by diluting the reagent with distilled water.

(by

B-1.1.2.1

volume).

B-1.1.2.2

Hydrochloric

Sulphuric

acid

1:2,

1:9,

1:19

acid —

1:1 (by volume).

B-1.1 .2.3 Hydrof7uoric

acid 1:3 (by volume).

B-1.1.3 Sodium Hydroxide

Dissolve 160 g of sodium hydroxide

up to 1000 ml. Store in a polyethylene flask.

Solution

in water and make

4

mol/1

B-1. 1.4 Polyethylene Oxide Solution — Dissolve 0.25 g of polyethylene oxide of average modular mass

200000

vigorously. This solution is stable for approximately

two weeks.

to 600000,

in

100 ml

water

while

stirring

Acid

Solution

Saturated

Dissolve

B-1. 1.5 Boric approximately

50

g of boric

acid

in water

and make

up to

1 000

ml.

B-1. 1.6 Potassium

Hydroxide

Solution

Dissolve

250 g of potassium hydroxide to 1 000 ml.

in water

and make

up

B-1.1.7 Citric Acid Solution — Dissolve 10 g of citric

up to

acid

in water

and make

100 ml.

B-1. 1.8,4 mmonium

A401ybdate

Solution

Dissolve

10 g of ammonium

molybdate

in water

and makeup

to

100 ml.

B-1.1.9 Reducing Solution — Dissolve in water 0.15 g of 1-amino-2 -hydroxy naphthalene-4 sulfonic acid

(C,0HgN04S), 0.7 g of sodium sulphite (anhydrous Na2S03) and 9 g of sodium metabisulphite (Na2S205) and make up to 100 ml. This solution will keep for a maximum of one week.

B-1.1.1O

Buffer

Solution

of pH

1.40

Dissolve

7.505

g

of

amino-acetic

acid

(NH2CHZCOOH)

and

5.850

g of sodium

chloride

in water

and make

up

to

1000

ml. Dilute

300

ml of this

solution

to

1000

ml

with dilute

hydrochloric

acid ( 1:99).

B-2 DETERMINATION

B-2.1

Decomposition

with

OF SILICA

Sodium

Peroxide

Weigh ( 1 0.05 g) of cement (ml) and 2 g of sodium peroxide into a platinum crucible and mix thoroughly with a spatula. Brush back into the mixture any particles adhering to the spatula. Cover the mixture with 1 g of

5

 

IS 3812

(Part

1) :2003

sodium

peroxide.

Carefully

preheat

the

covered

crucible

for about

2 min at the opening

of the furnace

 

before

placing

it

in

the

heated

zone

controlled

at

a

uniform

temperature

of (500

+ 10°C).

After

30 rein,

remove

cool to room temperature.

not

repeat

first

400 ml beaker

water.

until

cautiously

that

was

the crucible

stick

to the sides

from

the decomposition

Cover

the

solid

used.

the furnace

The

sintered

and allow mass If it does,

mass

Then

it to

should

to

a

of the crucible.

Transfer

the

then

at a temperature 10“C lower

sintered

with

glass

The

and rin~e the crucible

the beaker

with

is completely

150 ml cold

and heat

add

a watch

dissolved.

acid.

50 ml of hydrochloric

solution

obtained

repeat

increased

Add to the solution

the solution to the boil and boil for 30 min.

shall

be perfectly

clear.

If not,

reject

it and

the decomposition

by peroxide at a temperature

by 10°C or for double the time in the furnace.

1 ml of sulphuric

acid ( 1:1). Bring

B-2.2

Precipitation

B-2.2.1

Procedure

and Determination

of Silica

Evaporate

to cool. Treat the residue

of hydrochloric

to dryness the solution and allow the beaker

with 5 ml of water

and

10 ml

acid. While stirring, add some ashless

filter

paper

pulp

to the mixture

and

then

5

ml

of the

polyethylene

oxide

solution

ensuring

that

the

precipitate

and the polyethylene

oxide are thoroughly

mixed,

especially

the precipitate

adhering

to the sides

of the

beaker.

Stir

the

mixture

thoroughly

 

then

add

10 ml of water,

stirring

briefly

and leave

to stand

for

5 min. Then filter through

a mediumfilter

paper

into a

500

ml volumetric

flask and rinse with hot hydrochloric

acid

(1: 19). Remove

-any precipitate

adhering to

the

sides

of the beaker

using

a rubber

scraper.

Wash

the

filter

and

precipitate

at least

five

times

with

hot

hydrochloric

acid

(1: 19), then

rinse

with

hot water,

ensuring

that

the

residue

in the

filter

is broken

up

thoroughly

during

washing,

until

free

from

Chloride

ions.

Collect

the

washings

in

the

same

500

ml

volumetric

flask. Ignite

the filter and the precipitate

in

a platinum

crucible.( 1 175 + 25°C). Check for constant

mass m2.

B-2.2.2

Expression

of Results

The

impure

silica

is calculated

in percent

from

the

following

formula:

 

where

ml

m2

Impure

SiOl

= ~

W

x 100

=

mass

of the test portion,

in g;

and

=

mass determined

in accordance

with B-2.2.1,

in g.

1S 3812

(Part

1) :2003

B-2.3

Determination

B-2.3. 1 Procedure

of Pure

Silica

Moisten the residue obtained with about 0.5 ml to 1 ml of water. Add approximately 10 ml of hydrofluoric acid and then two drops of sulphuric acid. Evaporate

then

in a fume cupboard over

a sand bath or hot plate,

B-2.5

Determination

‘B-2.5.1 Procedure

of Soluble

Silica

Pipette 20 ml of the solution prepared in accordance with B-2.4 from the 500 ml volumetric flask into a polyethylene beaker already containing a magnetic stirrer bar and add 20 ml water. While stirring with

cent inue to heat until free from white sulphuric acid

the magnetic

stirrer,

add

15 drops

of hydrofluoric

acid

fumes.

Ignite the crucible

with the evaporationresidue

(1 :3). Stir again

for at least

1 min. Then

pipette

15 ml

in an electric

to cool to room temperature in a desiccator and weigh (ml). The evaporation residue is decomposed as

described in %2.4. If the residue obtained by this method exceeds 0.5 percent, the analysis shall be restarted and decomposition with sodium peroxide used.

furnace

(1

175 + 25”C)

for 10 rein, leave

B-2.3.2

Expression

of Results

The pure silica content is calculated the following formula:

in percent

from

where

Pure

Si02

=~x100

ml

ml

=

mass

of the test portion,

in g,

m,

=

mass determined

 

in

accordance

with

 

B-2.2.1,

in

g,

and

m,

=

mass

determined

in

accordance

with

 

B-2.3.1,

in

g.

B-2.4

Decomposition

of the

Evaporation

Residue

To the

evaporation

residue,

obtained

in accordance

with

sodium

using

the

that no part of the residue

B-2.2.1,

residue

add

2

g

of

mixture

Swirl

burner.

is completely

the

sodium

carbonate

and

red heat

until

chloride

a gas

and fuse to a bright

the

melt

frequently

dissolved. Check visually

remains

at the base

of the

crucible.

Allow

the crucible

and its contents

to cool,

transfer

to

a 250

ml beaker,

add

about

100 ml water

and

acidify

with

a

few

ml

of

concentrated

hydrochloric

completely dissolved, remove the platinum crucible

acid.

When

the

decomposed

mass

is

from the solution

and rinse it with water. The solution

shall be perfectly

clear. If not, filter through a medium

filter

paper,

wash,

bum

off the paper,

ignite

and then

repeat

the

decomposition

as

above.

Transfer

the

solution

to the

500

ml

volumetric

flask

containing

the

silica in accordance with B-2.2.1. Fill the flask up to

the

of

filtrate

mark

and

with

washings

water.

from

the

precipitation

this

solution

After

stirring,

is

ready

for use. It is used

in the photometric

determina-

tion of the silica remaining in solution

(see B-2.5)

oxide, aluminium oxide, calcium oxide and magnesium

oxide.

of the boric acid solution.

to (1.15 * 0.05) by adding, drop by drop, sodium

hydroxide

calibrated with a buffer solution of similar pH value

(for example 1.40). Add from a pipette 5 ml of the

ammonium molybdate solution to the solution (time O).

Adjust the pH of the solution

hydroxide

by drop, the sodium

acid (1:2). Transfer the solution to a 100 ml volumetric

Adjust

thepH

of the solution

meter

or hydrochloric

acid ( 1:2), using apH

to 1.60 by adding,

drop

solution or hydrochloric

flask and rinse the beaker with hydrochloric acid of

pH

citric acid solution, stir and leave to stand for 5 min. Then add from a pipette 2 ml of the reducing solution. Make up to volume with dilute hydrochloric acid of pH 1.60 and mix. At time O + 30 min measure the optical density with the photometer against a blank solution prepared in a similar way and using the same wavelength of a cell of the same optical length as used

1.60. After

20 rein,

add from

a pipette

5 ml

of the

The silica

concentration in mg SiOz per 100 ml is read from the

for the construction

of the calibration

graph.

calibration graph (md).

B-2.5.2

Expression

of Results

The soluble silica content is calculated in percent from the following formula:

where

Soluble SiOz

500xm,

20xltlt10xml

x100

m,

=

mass of the test portion, in g; and

md

=

silica content of the solution in accordance with B-2.5 in mg Si02/100 ml.

B-2.6

Total

Silica

 

B-2.6.1

Expression

of Results

The total silica content

is equal

to the sum

of the pure

silica content

(see B-2.3)

and the soluble

silica content

(see B-2.5).

B-3

RESIDUE

DETERMINATION

OF

INSOLUBLE

B-3.1

Procedure

 

To

(1

+ 0.05

g) of cement

(mJ,

placed

in a porcelain

 

dish,

add

25

ml

of cold

water

and

disperse

using

a

6

IS 3812

(Part

1) :2003

glass stirring

rod. Add 40 ml of hydrochloric

acid. Heat

mass (mG). In general,

an ignition

period

of 30 min

is

the solution gently and crush the sample with the

sufficient

for obtaining

constant

mass.

flattened

end of a glass stirring

rod until decomposition

 

of the cement is complete. Evaporate to dryness on a

B-3.2

Expression

of Results

 

water bath. Repeat the operation twice more with 20 ml

The insoluble

residue

is calculated

in percent

from the

hydrochloric acid. Treat the residue from the last

following

formula:

evaporation with 100 ml of dilute hydrochloric acid

and

wash with almost

free

contents to a 250 ml conical flask fitted with a bulb condenser and add 100 ml of the potassium hydroxide solution. Leave to stand for 16 h at room temperature and then boil the solution under reflux for 4 h. Filter on a medium filter paper and wash with water then with 100 ml of hydrochloric acid ( 1:9) and finally with almost boiling water until free from Chloride ions. Ignite at (975 + 25”C) then check for constant

its

(1 :3). Re-heat

filter through

boiling

ions.

a medium

filter paper

water

at least ten times until

the -filter

and

from

Chloride

Transfer

where

Insoluble

residue

=

ax

m5

100

m~

=

mass

of the test portion,

in g;

and

mb

=

mass

of the ignited

insoluble

residue,

in g,

B-4 REACTIVE

SILICON

DIOXIDE

(Si02)

This is determined by subtracting from total silicon dioxide content (see B-2.6) that fraction contained in the insoluble residue (see B-3) both on dry sides.

7

IS 3812

(Part

1) :2003

ANNEX

(Foreword)

C

 

COMMITTEE

COMPOSITION

 

Cement

and Concrete

Sectional

Committee,

CED

2

Orgunizalioti

Representative(s)

[II personal

capacity

( ‘Chandrika’,

at

15(II Cross

63-64

Easf Park

DR H. C. VISVESVARAYA(Chairman)

 

Rmid

Mullcwaram,

Batlgalore-560

003)

B.

(i.

Shirke